固载型杂多酸催化剂制备及催化环己烯环氧化工艺研究-化学工艺专业论文.docxVIP

摘要摘要 摘要 摘要 本文，对固载型磷钨杂多酸季铵盐催化剂的制备工艺及其催化过氧化氢环 氧化环己烯合成环氧环己烷的工艺过程进行了研究，其主要研究内容如下： 对现有该固载型催化剂的制各工艺进行改进：通过调整加料比，提高原料 利用率，大大降低了生产成本；选用浓度为C3的A酸制备中间产物钨酸，不仅 简化了实验操作，而且可使催化剂内部形成酸性环境，有助于增强其催化活性； 调整磷酸加入量并改进加料方式，得到W／P比为4的催化剂活性组分 {e04[wo(02)2]4)3-，其在载体上负载率为38％。 将制备出的固载型磷钨杂多酸季铵盐催化剂用于环己烯环氧化合成环氧环 己烷反应，对其催化性能进行了评价，利用气相色谱采用内标法对产物进行定 量分析，并对反应前后催化剂的结构进行了红外表征，结果表明该催化剂结构 稳定，重复使用十次后，仍可保持较好的催化性能，可多次重复使用。 对影响环氧环己烷合成反应的主要因素进行了考察，如助剂加入量、催化 剂处理方式、反应温度、反应时间、催化剂用量等，优化得到了较佳的合成工 艺条件：无溶剂，环己烯与过氧化氢摩尔比为1．75：1，过氧化氢水溶液226．69， 催化剂329，助剂10．679，无溶剂，反应温度为55℃，反应时间为5．5h，在较 佳工艺条件下，环己烯当量转化率可达85．5％，环氧环己烷选择性为95．4％。 在催化剂制备和环氧环己烷合成小试实验的基础上，设计放大实验，考察 了各自放大实验的可行性，为其规模化生成提供了依据。 关键词：磷钨杂多酸季铵盐；固载；环氧环己烷；环氧化 AbstractAbstract Abstract Abstract 111 this work，chloromethylated polystyrene(chlorine ball)grafted quaternary ammomum heterophosphortungstate catalyst was prepared and used in the epoxidation of cyclohexene oxidized by hydrogen peroxide．The main aspects of work were carried out as follow： Improvmg the existing technology of the preparation of immobilized catalsts through the following aspects：1)adisuting the ratios of feeds，this could improve the efficiency of raws and reduce the cost of production significantly；2)selecting acid A of C；concentration as acidifie synthesized H2W04．In this way,it simplified the experimental operation and also produced a quite special acid environment within the catalyst that enhanced its catalytic activity；3)adisuting the quantity of H3P04 and its feeding method，SO the active component{P04[WO(02)214}3 could been prepared， and its quotiety of cross—linking Was about 3 8％． Catalst Was used in the epoxidation of cyclohexene，we could carry out quantitative analysis of the product through gas chromatograph5 by intemal standard method，calculated based on cyclohexene．The equivalent coversion of cyclohexene Was 85．5％谢th 95．4％selectivity of epoxycyclohexan．And the structures of the fresh and recycled were characterised by IR spectroscopy,that indicated there was not much formation of structural tra